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At least 703 records · Page 39

High temperature steam oxidation of Cr-coated SiCf/SiC composite for LWR cladding applications

Chromium-coated silicon carbide fiber-reinforced ceramic matrix composites are potentially applicable to accident tolerant fuel cladding in light water reactors. Cr-coated silicon carbide composite, chemical vapor deposited silicon carbide, and pure Cr-metal were oxidized in 100% steam at atmospheric pressure for 4 hours using a thermogravimetric analyzer. Post-oxidation chemical analysis, phase identification and microstructural characterization indicates that the Cr coating layers did not adversely affect silicon carbide substrate under these conditions.

Lee, Yoonjo↗

DED Additively Manufactured HEAs Optimized via Parametric Study of Functionally Graded Materials

Complex concentrated alloys (CCAs) are a system of alloys composition of nearly equiatomic elements, creating a state of high configurational entropy in the material. These alloys are of interest for various industrial applications due to their high strength and hardness, wide operational temperature range, creep and diffusion resistance, and radiation resistance. In the current work CoCrFeNi-base CCAs are synthesize by combining three commonly industrial alloys: IN718, SS316L, and 70Co30Cr (commercially known as Stellite 21), in-situ utilizing directed energy deposition (DED) additive manufacturing (AM). One bulk specimen is fabricated with a 1:1:1 ratio of IN718, SS316L, and 70Co30Cr where IN718 is a source of nickel and chrome, SS316 is a source of iron and chrome, and 70Co30Cr is a source of cobalt and supplemental chrome. Additionally, a functionally graded material (FGM) of the identified CCA system from SS316 was fabricated with 10 layers, where the initial five layers are the base material of SS316L and graded by steps of 20% to transition to the CCA system. Overall build quality, microstructure, compositional distribution, phases analysis, and microhardness were studied by laser optical microscopy, scanning election microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction analysis (XRD), and Vickers microhardness techniques. Overall build quality showed a successful bulk build with acceptable density, however unmelted particles are observed in the as-built alloy. Compositional results show that the system meets the Boltzmann’s hypothesis definition of an HEA, and that an FCC CCA was produced with increased hardness, small grain size, and superior hardness properties to the SS316L substrate. While initial XRD results show predominately FCC structure, EDS analysis of interdendritic regions show the existence of Laves phases in the material. The fabrication of an FGM CCA allowed for potential screening of additional alloy mixes which may be of interest to explore in future research, and the resulting composition is compared to predicted values. This novel method of CCA fabrication results in substantial cost savings of these CCA systems over traditional methods.

36 MATERIALS SCIENCE↗

Microstructures of chemical vapor deposited high-purity tungsten achieved by two different precursors

Highlights: • CVD tungsten used as electron emitters of thermionic fuel elements was investigated. • Microstructures were characterized with metallography analysis. • The preferred orientation was determined with XRD and EBSD. • The surface morphology was observed with SEM and WLI. • Tungsten via thermolysis of WCl{sub 6} is better for thermionic fuel elements. - Abstract: Chemical vapor deposited (CVD) high-purity tungsten can be manufactured as electron emitters in thermionic fuel elements. Exposed surface planes of the emitter emit electrons and affect the efficiency and load capacity of the thermionic fuel element. In order to determine the electron emission planes of the emitter, the metallurgic structures, the preferred orientation and the as-deposited surface morphology of CVD tungsten have been investigated. In this work, high-purity (over 99.99%) tungsten was achieved by two different precursors: hydrogen reduction of tungsten hexafluoride (WF{sub 6}) and thermolysis of tungsten hexachloride (WCl{sub 6}). The microstructures of CVD tungsten were characterized by metallography analysis, X-ray diffraction (XRD), electron backscattered diffraction (EBSD), and white light interference (WLI). Tungsten fabricated by hydrogen reduction of WF{sub 6} and thermolysis of WCl{sub 6} has <100>-preferred columnar microstructures. However, the latter exhibits larger columnar grains and preferred <100> less. The preferred orientation is caused by the higher growth rate of the <100> orientation and competition between the <100> orientations of different grains. The as-deposited surface consists of tiny pyramids, with <100> axis and {111} side faces. In contrast to tungsten produced by hydrogen reduction of WF{sub 6}, the pyramid on tungsten synthesized via thermolysis of WCl{sub 6} contains small {110} facets on the four edges. Therefore, tungsten made via thermolysis of WCl{sub 6} is a better candidate for thermionic fuel elements, because the higher work function of {110} planes enables better output efficiency.

36 MATERIALS SCIENCE↗

Characterization of Mechanical Performance of Composites Fabricated Using Innovative Carbon Fiber Wet Laid Process

Recent innovation in production of optimized nonwoven wet laid (WL) carbon fiber (CF) mats raised the question of optimal translation of the performance and isotropy into composites formed through these dry preforms. This work explores the mechanical behavior of composites produced from WL-CF mats in conjunction with the microstructure predicted through Object Oriented Finite Element Analysis (OOF). The mats used for the composites were prepared in two dispersion regimes using 25.4 mm long CF. The mixing regimes discussed in the author’s previous work, are identified as Method 1 for the traditional processing regime and Method 2 for the innovative regime that provided optimal nonwoven WL-CF mats. Composite panels from Method 2 mats showed a normalized tensile strength increase of 52% over those from Method 1 panels. Reproducibility analysis of composites made from Method 2 mats demonstrated a standard deviation of 2% in fiber weight content, 2% in tensile modulus and 9% in tensile strength, while composites made from Method 1 mats demonstrated a standard deviation of 5% in fiber weight content, 5% in tensile modulus and 17% in tensile strength. Systematic study of the microstructure and its analysis through OOF confirmed the isotropy translation of mats produced through method 2 to the composites. This study validated the hypothesis that optimal nonwoven mats lead to a well-balanced composite with optimal performance and that non-optimal nonwoven mats do not pack into a well-balanced composite.

36 MATERIALS SCIENCE↗

Archaeometallurgical investigation of the iron anchor from the Tantura F shipwreck

The Tantura F shipwreck was a coaster or a fishing vessel about 15.7 m long, discovered in the Dor/Tantura lagoon, Israel in 1995. It was dated to between the mid-7th and the end of the 8th centuries CE. Among the finds excavated were two T-shaped type iron anchors. Of the two anchors, one (anchor A) was thoroughly studied by archaeometallurgical methods in order to identify forge-welding lines, to determine the welding quality and to understand the manufacturing technology. The examinations included X-ray radiography, XRF analysis, optical microscopy, SEM/EDS observation and analysis, OES analysis and microhardness tests. The investigation included characterization of the composition, microstructure, thermal treatments, forge-welding junctions and slag analysis. The results revealed a heterogeneous microstructure, rich in glassy, fayalite and wüstite slag. Iron based phases included ferrite, pearlite, cementite and Widmanstätten plates, all typical to wrought iron. The forge-welds of Anchor A were located. Each arm was made of one piece, weighing about 2.5–3 kg and the shank was made of a few 1.5–2 kg pieces. The second anchor (anchor B) was only briefly examined visually and with a few radiographs, which support the results from anchor A. The research results revealed significant information about T-shaped anchors and their manufacturing process, including hot-working processes without any additional heat treatments, and folding techniques. The microstructure was similar to other ancient simple tools such as saws, sickles, axes and mortise chisels, and though the technology to make complicated structures and objects, such as swords, existed at that time, the anchors did not require this sophistication; thus simpler techniques were used, presumably because they were more cost-effective. - Highlights: ► Tantura F was a coaster dated to mid-7th–end-8th centuries. ► Two iron anchors were discovered at the Tantura F shipwreck-site. ► Anchor A was manufactured from heterogeneous wrought iron blooms. ► Forge-welding lines were detected using archaeometallurgical methods.

36 MATERIALS SCIENCE↗

Preliminary characterization and projections of PVD coatings on SiC cladding for Light Water Reactors

Physical Vapor Deposition (PVD) based CrN, Cr and TiN are currently the leading mitigation coatings for SiC-based Light Water Reactor (LWR) fuel cladding. This manuscript describes the morphology, phase analysis and elemental composition of coatings deposited by commercial vendors on SiC clad materials. The coatings showed continuous crack-free morphology with few microstructural flaws. X-ray analysis and spectroscopy indicated high purity >99.9%. Mechanical tests of coating debonding (by ASTM D4541) and scratch-indentation (by ASTM E2546) were conducted. Strong interface bonding was observed and higher resistance to normal and shear stresses was observed from thicker coatings. Preliminary developments in scratch testing, phase analysis, future needs and expected behavior under irradiation are discussed.

Ang, Caen K.↗

Supercritical, liquid, and gas CO 2 reactive transport and carbonate formation in portland cement mortar

In this paper, we investigate carbonate formation and reactive transport rate in variably saturated portland cement mortars when high concentrations of gas, liquid, or supercritical CO 2 flow through their pore network. Xray computed tomography completed during CO 2 flow is used to quantify the microstructural evolution as the mortar carbonates. After in situ tests, higher resolution scans, thermogravimetric analysis, and desorption isotherm analysis are performed to further quantify microstructural changes. We found that at dry conditions supercritical CO 2 moves more rapidly through the pore space and precipitates more carbonates than liquid or gas CO 2 . However, at 50% degree of saturation (DOS) the CO 2 state did not affect the rate of transport in that each specimen exposed to a different CO 2 state carbonated within the first hour of CO 2 exposure. When the pore space is at 50 or 100% DOS, supercritical CO 2 did not react with hydration products more rapidly nor did it result in more carbonate formation during exposure compared to gas or liquid CO 2 . The amount of Ca(OH) 2 that contributes to CaCO 3 formation is correlated to the DOS. For the mortar composition analyzed, Ca(OH) 2 contributes to approximately 40% of the carbonates formed in the 50% DOS specimens and 15% in the 100% DOS specimens. In other words, as the amount of moisture in the pore space increases, phases other than Ca(OH) 2 contribute to more than 50% of the total CaCO 3 formed.

42 ENGINEERING↗

Quantitative Characterization of the Microstructure-Property Relationships in Ni and MIEC Nanocatalyst-Infiltrated Ni/YSZ Anodes

The performance of solid oxide fuel cell (SOFC) anodes can be improved by infiltration of nanoscale electrocatalysts, which increases triple phase boundary (TPB) density, but only when the added TPBs are active. Quantitative characterization of the microstructure of infiltrated nanocatalysts remains a critical challenge in understanding their role in improved performance. This paper explores the relationship between electrochemical performance and microstructure for Ni/YSZ anodes infiltrated with Ni, gadolinium-doped-ceria (GDC), and Ni/GDC nanocatalysts using a combination of electrochemical impedance spectroscopy (EIS), distribution of relaxation times (DRT) analysis, scanning electron microscopy (SEM) microstructural characterization, and three-dimensional (3-D) anode reconstruction. Estimated polarization resistance improvements as a result of nickel nanoparticle infiltration are discussed.

Rix, Jillian↗

Microstructure of calcite deformed by high-pressure torsion: An X-ray line profile study

Calcite aggregates were deformed to high strain using high-pressure torsion and applying confining pressures of 1–6 GPa and temperatures between room temperature and 450 °C. The run products were characterized by X-ray diffraction, and key microstructural parameters were extracted employing X-ray line profile analysis. The dominant slip system was determined as r {$ 10\bar{1}4 $}&lang;$ \bar{2}021 $&rang; with edge dislocation character. The resulting dislocation density and the size of the coherently scattering domains (CSD) exhibit a systematic dependence on the P-T conditions of deformation. While high pressure generally impedes recovery through reducing point defect mobility, the picture is complicated by pressure-induced phase transformations in the CaCO 3 system. Transition from the calcite stability field to those of the high-pressure polymorphs CaCO 3 - II, CaCO 3 - III and CaCO3-IIIb leads to a change of the microstructural evolution with deformation. At 450 °C and pressures within the calcite stability field, dislocation densities and CSD sizes saturate at shear strains exceeding 10 in agreement with earlier studies at lower pressures. In the stability field of CaCO 3 - II, the dislocation density reflects a more complex behavior. Furthermore, at a given strain and strain rate, the dislocation density increases and the CSD size decreases with increasing pressure within the stability fields of either calcite or of the high-pressure polymorphs. There is, in contrast, a jump from high dislocation densities and small CSDs in the upper pressure region of the calcite stability field to lower dislocation densities and larger CSDs in the low-pressure region of the CaCO 3 - II stability field. This jump is more pronounced at higher temperatures and less so at room temperature. The pressure influence on the deformation-induced evolution of dislocation densities implies that pressure variations may change the rheology of carbonate rocks. In particular, a weakening is expected to occur at the transition from the calcite to the CaCO 3 - II stability field, if aragonite does not form.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reconstructing parent microstructures in martensitic and pearlitic Ti-Cu

Evaluating the microstructural evolution of parent phases has long been a challenge in metals with a partial or complete solid state transformation. Most parent microstructure evolution has to be inferred from the product microstructure, with some information permanently lost. Parent microstructure reconstructions relying on orientation relationships and EBSD data are a useful tool to overcome this challenge, though much background knowledge is required to do so. Here, this work introduces a reconstruction process for a eutectoid composition Ti-Cu binary alloy to evaluate the high temperature β-Ti phase from martensitic and pearlitic product microstructures. Martensitic microstructures were accurately reconstructed, enabling elucidation of β-Ti grain size and texture, and the employed script included for scientific reference. Pearlitic microstructures did not reconstruct effectively with the current process. However, new insight into the interfacial crystallographic orientations of pearlitic Ti-Cu microstructures was gleaned via this analysis, and future investigations of interest are discussed accordingly. Ultimately, these findings demonstrate tools widely implemented on conventional titanium and ferrous alloys can also be applied to understand parent microstructures in Ti-Cu and other alloys of emerging interest. This is especially of use as new manufacturing processes for such materials require understanding how parent phase microstructures respond to new, novel material processing such as AM.

36 MATERIALS SCIENCE↗

Liquid immiscibility and core-shell morphology formation in ternary Al–Bi–Sn alloys

The effects of composition on liquid immiscibility, macroscopic morphology, microstructure and phase transformation in ternary Al–Bi–Sn alloys were investigated. Three types of morphology, the core-shell type, the stochastic droplet type and uniform dispersion type, of Al–Bi–Sn particles prepared by a jet breakup process were distinguished, and the relationships between which were discussed. The phase transformation behaviors of the Al–Bi–Sn alloys were studied by thermal analysis, in agreement with the microstructural observation and microanalysis. The liquid immiscibility and formation of the core-shell morphology in Al–Bi–Sn alloys are easily achieved when the composition lies in the liquid miscibility gap. The particles exhibit a high melting point Al-rich core with a low melting point Sn–Bi-rich solder shell, showing promise for application as high-density electronic packaging materials. - Highlights: • The liquid demixing, morphology and microstructure in Al–Bi–Sn alloys were studied. • Three types of morphology were classified and discussed. • The conditions for formation of the core-shell morphology were obtained. • The phase transition behaviors agree with the microstructure characterization. • The Al/Sn–Bi core-shell particles show promise for use in electronic packaging.

36 MATERIALS SCIENCE↗

Structural, microstructural and thermal properties of lead-free bismuth–sodium–barium–titanate piezoceramics synthesized by mechanical alloying

Graphical abstract: Mechano-synthesis of lead-free (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} piezoceramics with nanocrystalline/amorphous structure and homogeneous composition: partial transformation of constituents to BNBT, BNT and pyrochlore, amorphous phase formation, mechano-crystallization of the amorphous, pyrochlore-to-perovskite BNBT phase transformation during the process. Display Omitted Highlights: ► Perovskite BNBT powders with homogeneous composition were synthesized by MA. ► Partial transformation of constituents to BNBT, BNT and pyrochlore occurred by MA. ► Formation of an amorphous phase and afterwards its crystallization occurred by MA. ► Pyrochlore-to-perovskite BNBT phase transformation occurred after prolong milling. ► Polymorphic transformations of TiO{sub 2} act as the main alloying impediment during MA. -- Abstract: Bismuth–sodium–barium–titanate piezoceramics with a composition of (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} (BNBT) were prepared by mechanical alloying (MA). Structural analysis and phase identification were performed by X-ray diffraction (XRD). Microstructural studies and chemical composition homogeneity were performed by scanning electron microscope (SEM) coupled with energy dispersive X-ray analysis (EDX). Furthermore, thermal properties of the as-milled powders were evaluated by thermogravimetry/differential thermal analysis (TG/DTA). During the initial milling, the constituents were transformed to the perovskite, pyrochlore, and BNT phases; in addition, partial amorphization of the structure appeared during the milling cycle. As MA progressed, transformation of pyrochlore-to-perovskite and crystallization of the amorphous phase occurred and also, the BNBT phase was significantly developed. It was found that the MA process has the ability to synthesize the BNBT powders with a submicron particle size, regular morphology, and uniform elemental distribution.

36 MATERIALS SCIENCE↗

Quantitative assessment of particle dispersion in polymeric composites and its effect on mechanical properties

In this work, an automated image analysis tool is developed to establish quantitative correlations between the particle/cluster size distribution and the mechanical properties of particle reinforced polymer composites (PRPC).This automated image analysis tool is developed within python programming software to process and analyze the microstructural images of the polymerbased composite materials. The spent coffee bean powder (SCBP) reinforced poly-propylene carbonate (PPC) polymer composite with differing wt.% of the filler is selected for the analysis. Detailed statistical analysis of the microstructural images reveals that ‘clustering of clusters’ is also presented in addition to the most commonly reported ‘clustering of particles’, and the distribution of particle/clusters is bimodal. Based on these findings, an effective volume fraction for the filler material is proposed to mainly capture the agglomeration effect. With this effective volume fraction, the standard rule-of-mixture model correctly captures the experimentally measured tensile strength and modulus as a function of filler wt.%. Further, the applicability of this effective volume fraction for other theoretical models is also analyzed. The detailed statistical analysis of the microstructure and the proposed effective volume fraction helps to develop a deeper quantitative understanding of the PRPC than the conventional qualitative correlation of microstructural features with the properties and failure processes.

36 MATERIALS SCIENCE↗

Characterization of High Temperature Mechanical Properties Using Laser Ultrasound

Mechanical properties are controlled to a large degree by defect structures such as dislocations and grain boundaries. These microstructural features involve a perturbation of the perfect crystal lattice (i.e. strain fields). Viewed in this context, high frequency strain waves (i.e. ultrasound) provide a natural choice to study microstructure mediated mechanical properties. In this presentation we use laser ultrasound to probe mechanical properties of materials. This approach utilizes lasers to excite and detect ultrasonic waves, and as a consequence has unique advantages over other methods—it is noncontacting, requires no couplant or invasive sample preparation (other than that used in metallurgical analysis), and has the demonstrated capability to probe microstructure on a micron scale. Laser techniques are highly reproducible enabling sophisticated, microstructurally informed data analysis. Since light is being used for generation and detection of the ultrasonic wave, the specimen being examined is not mechanically coupled to the transducer. As a result, laser ultrasound can be carried out remotely, an especially attractive characteristic for in situ measurements in severe environments. Several examples involving laser ultrasound to measure mechanical properties in high temperature environments will be presented. Emphasis will be place on understanding the role of grain microstructure.

36 MATERIALS SCIENCE↗

Multiscale mechanical behavior and microstructure evolution of extruded magnesium alloy sheets: Experimental and crystal plasticity analysis

Highlights: • Experimental stress-strain responses were reproduced by CPFE simulation based on Voronoi grains on three strain paths. • Textures predicted by simulation were in accordance with the ones measured by EBSD at the strain of 0.085. • Deformation heterogeneity in slip-dominated cases was found more significant than that in twin-favored case. • For slip-dominated cases, both high m′ value and high SFs in adjacent grains are responsible for strain localization. - Abstract: A phenomenological crystal plasticity finite element (CPFE) model based on Voronoi grains was applied to reproduce basic deformation features of a hot-extruded magnesium alloy sheet under various strain paths. Corresponding experimental investigations, including mechanical tests, electron back scattered diffraction (EBSD) measurements and optical observation, were also carried out as either a validation or a supplement of the numerical results. Predicted average stress-strain responses and texture evolution are in good accordance with measured ones. Furthermore, deformation heterogeneity at the mesoscopic and intergranular scale were investigated based on the proposed model. At the mesoscale, the heterogeneity in the slip-dominated cases tends to develop continuously, whereas the heterogeneity is retarded in twin-favored deformation. At the intergranular scale, it is concluded from the slip-dominated case that a high slip-transfer parameter and high Schmid factors (SFs) of principal slip systems in adjacent grains could accommodate higher local strain.

36 MATERIALS SCIENCE↗

Analysis of thermal history effects on mechanical anisotropy of 3D-printed polymer matrix composites via in situ X-ray tomography

The tensile behavior of an additively manufactured (AM) polymer matrix composite (PMC) is studied with in situ X-ray computed microtomography (CT) and digital volume correlation (DVC). In this experiment, the effects of recycled material content and print direction on the selective laser-sintered (SLS) material's mechanical response are explored. The PMC samples are printed in a tensile specimen geometry with gage lengths parallel to all three orthogonal, primary sintering directions. In situ tensile-CT experiments are conducted at Argonne National Laboratory's Advanced Photon Source 2-BM beamline. Analysis of the AM PMC's tensile response, failure, and strain evolution is analyzed both from a conventional standpoint, using the load-displacement data recorded by the loading fixture, and from a microstructural standpoint by applying DVC analysis to the reconstructed volumes. Significant variations on both strength and ductility are observed from both vantages with respect to print direction and the recycled material content in the printed parts. As a result, it is found that the addition of recycled source material with a thermal history reduces the tensile strength of the SLS composite for all directions, but the effect is drastic on the strength in the layering direction.

36 MATERIALS SCIENCE↗

Influence of the interface structure on the thermo-mechanical properties of Cu-X (X = Cr or B)/carbon fiber composites

Highlights: Black-Right-Pointing-Pointer Two copper alloys/carbon fibers composites have been produced. Black-Right-Pointing-Pointer Correlation of the thermo-mechanical properties with the microstructure and the chemistry. Black-Right-Pointing-Pointer A composite with CTE 25% lower than a classic Cu/CF composite has been obtained. -- Abstract: This study focuses on the fabrication, for power electronics applications, of adaptive heat sink material using copper alloys/carbon fibers (CF) composites. In order to obtain composite material with good thermal conductivity and a coefficient of thermal expansion close to the ceramic substrate, it is necessary to have a strong matrix/reinforcement bond. Since there is no reaction between copper and carbon, a carbide element (chromium or boron) is added to the copper matrix to create a strong chemical bond. Composite materials (Cu-B/CF and Cu-Cr/CF) have been produced by a powder metallurgy process followed by an annealing treatment in order to create the carbide at the interphase. Chemical (Electron Probe Micro-Analysis, Auger Electron Spectroscopy) and microstructural (Scanning and Transmission Electron Microscopies) techniques were used to study the location of the alloying element and the carbide formation before and after diffusion. Finally, the thermo-mechanical properties have been measured and a promising composite material with a coefficient of thermal expansion 25% lower than a classic copper/carbon heat sink has been obtained.

36 MATERIALS SCIENCE↗

Modeling of microstructural effects on electromigration failure

Current electromigration models used for simulation and analysis of interconnect reliability lack the appropriate description of metal microstructure and consequently have a very limited predictive capability. Therefore, the main objective of our work was obtaining more sophisticated electromigration tools. The problem is addressed through a combination of different levels of atomistic modeling and already available, continuum level macroscopic models. A novel method for an ab initio calculation of the effective valence for electromigration is presented and its application on the analysis of EM behavior is demonstrated. Additionally, a simple analytical model for the early electromigration lifetime is obtained. We have shown that its application provides a reasonable estimate for the early electromigration failures including the effect of microstructure. A simulation study is also applied on electromigration failure in tin solder bumps, where it contributed the understanding of the role of tin crystal anisotropy in the degradation mechanism of solder bumps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗